HRID2373213
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of ethyl 4-(3-chlorophenyl)-1-ethyl-6-methyl-4,7-dihydro-1H-pyrazolo[3,4-b]pyridine-5-carboxylate (135 mg) in THF (3 ml) was added 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (97.5 mg) and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into saturated NaHCO3 and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous MgSO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with a mixture of EtOAc and n-hexane (1:5) to give ethyl 4-(3-chlorophenyl)-1-ethyl-6-methyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate (47 mg) as colorless oil.
WORKUP
后处理
- extractionextracted with EtOAc
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by flash column chromatography on silica gel eluting with a mixture of EtOAc and n-hexane (1:5)